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Composition of extraction products from alkylated high-sulphur coals

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Central European Journal of Chemistry

Abstract

Products of reductive and non-reductive methylation of two high-sulphur coals (Mequinenza and Illinois No. 6) have been extracted by dichloromethane. It has been established that the efficiency of the transformation of coal to the products soluble in CH2Cl2 is higher for coals subjected to non-reductive methylation by the Liotta method than for those after reduction in the potassium/liquid ammonia system. The extracts and the extraction residues were subjected to elemental analysis, IR spectroscopy, and AP-TPR (Atmospheric Pressure-Temperature Programmed Reduction) measurements. It has been shown that the main species undergoing extraction by CH2Cl2 are aliphatic compounds or aromatic structures of low degree of condensation. The effect of the extraction on the sulphur groups in coal has been discussed.

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References

  1. L.M. Stock: “The Reductive Alkylation Reaction”, In: M.L. Gorbaty, J.W. Larsen, I. Wender (Eds.). Coat Science, Academic Press, Vol. 1, New York, 1982, pp. 161–282

  2. H. Wachowska and M. Kozłowski: “Multistage butylation of coals in a potassium-liquid ammonia system”, Fuel, Vol. 72, (1993), pp. 435–442.

    Article  CAS  Google Scholar 

  3. L. Lazarov, M.F. Simeonov, S.P. Marinov: “Structural analysis of alkylated coal by 1H and 13CNMR spectroscopy”, Fresenius Z. Anal. Chem., Vol. 319, (1984), pp. 552–555.

    Article  CAS  Google Scholar 

  4. H.W. Sternberg, C.L. Delle Donne, P. Pentages, E.C. Moroni, R.E. Markby: “Solubilization of an lvb coal by reductive alkylation”, Fuel, Vol. 50, (1971), pp. 432–442.

    Article  CAS  Google Scholar 

  5. K. Niemann and U.B. Richter: “Studies int he chemical characterization of coal: reduction”, Fuel, Vol. 58, (1979), pp. 838–840.

    Article  CAS  Google Scholar 

  6. M. Miyake, M. Sukigara, M. Nomura, S. Kikkawa: “Improved method to alkylate Yubari coal of Japan using molten potassium under refluxing THF”, Fuel, Vol. 59, (1980), pp. 637–640.

    Article  CAS  Google Scholar 

  7. M. Miyake, S. Yamamoto, M. Nomura: “Enhanced oil production from coal by a new reductive alkylation reaction in a glass flask”, Fuel Processing Technology, Vol. 14, (1986), pp. 201–211.

    Article  CAS  Google Scholar 

  8. L. Lazarov, I. Rashkov, S. Angelov: “Direct preparation of ionic potassium-coal adducts”, Fuel, Vol. 57, (1978), pp. 637–638.

    Article  CAS  Google Scholar 

  9. H. Wachowska and M. Kozłowski: “Studies of reduction and reductive alkylation of coals in the potassium/liquid ammonia system. 1. The influence of demineralization on the course of reduction and reductive alkylation of coals”, Fuel, Vol. 74, (1995), pp. 1319–1327.

    Article  CAS  Google Scholar 

  10. B.S. Ignasiak, J.F. Fryer, P. Jadernik: “Polymeric structure of coal. 2. Structure and thermoplasticity of sulphur-rich Raša lignite”, Fuel, Vol. 57, (1978), pp. 578–584.

    Article  CAS  Google Scholar 

  11. R. Liotta: “Selective alkylation of acidic hydroxyl groups in coal”, Fuel, Vol. 58, (1979), pp. 724–728.

    Article  CAS  Google Scholar 

  12. J.W. Larsen and E.W. Kuemmerle: “Alkylation and depolymerization reactions of coal: a selective review with supplementary experiments”, Fuel, Vol. 55, (1976), pp. 162–169.

    Article  CAS  Google Scholar 

  13. H. Wachowska, M. Kozłowski, J. Thiel, I. Dunajska-Szopka: “Studies of the effects of O-alkylation on the extractability of demineralized and reduced Polish coals”, Fuel Processing Technology, Vol. 29, (1991), pp. 143–151.

    Article  CAS  Google Scholar 

  14. B. Ignasiak, D. Carson, M. Gawlak: “Non-destructive solubilization of coal”, Fuel, Vol. 58, (1979), pp. 833–834.

    Article  CAS  Google Scholar 

  15. L.B. Alemany and L.M. Stock: “Reductive alkylation of Illinois No. 6 coal.1H and 13C n.m.r. spectra of the 13C-enriched alkylation products”, Fuel, Vol. 61, (1982), pp. 1088–1094.

    Article  CAS  Google Scholar 

  16. M. Kozłowski, H. Wachowska, P. Adriaensens, J. Gelan: “IR and NMR characterisation of extraction products of reductively deuteromethylated coals”, Fuel, Vol. 78, (1999), pp. 1881–1884.

    Article  Google Scholar 

  17. L. Lazarov and S.P. Marinov: “Modeling the structure of a coking coal”, Fuel Processing Technology, Vol. 15, (1987), pp. 411–422.

    Article  CAS  Google Scholar 

  18. M. Kozłowski, H. Wachowska, J. Yperman: “Reductive and non-reductive methylation of high-sulphur coals studied by atmospheric pressure-temperature programmed reduction technique”, Feul, Vol. 82, (2003), pp. 1041–1047.

    Article  Google Scholar 

  19. W. Radmacher and P. Mohrhauer: “Demineralizing of coal for analytical purposes”, Brennstoff-Chemie, Vol. 37, (1956), pp. 353–358.

    CAS  Google Scholar 

  20. Polish Standard PN-76/G-04514.02: “Solid fuels. Determination of total sulphur by the high-temperature combustion method”

  21. J. Yperman, I.I. Maes, H. Van den Rul, S. Mullens, J. Van Aelst, D.V. Franco, J. Mullens, L.C. Van Poucke: “Sulphur group analysis in solid matrices by atmospheric pressure-temperature programmed reduction”, Analytica Chimica Acta, Vol. 395, (1999), pp. 143–155.

    Article  CAS  Google Scholar 

  22. M. Kozłowski, H. Wachowska, J. Yperman, D.V. Franco, J. Mullens, L.C. Van Poucke: “Atmospheric-pressure temperature-programmed reduction study of high-sulfur coals reduced in a potassium/liquid ammonia system”, Energy & Fuels, Vol. 12, (1998), pp. 1142–1147.

    Article  Google Scholar 

  23. M. Avram and G.D. Mateescu: Infrared Spectroscopy, Robert E. Krieger Publishing Company, New York, 1978, pp. 323.

    Google Scholar 

  24. V.I. Stenberg, R.J. Baltisberger, K.M. Patal, K. Raman, N.F. Woolsey: “The role of noncovalent bonding in coal”, In: M.L. Gorbaty, J.W. Larsen, I. Wender (Eds.): Coal Science, Vol. 2, Academic Press, New York, 1983, pp. 125–171.

    Google Scholar 

  25. E. Yaĝmur, B. Çiçek, A. Olcay: “Effect of O-methylation on solubility and swelling of coals”, Fuel Processing Technology, Vol. 67, (2000), pp. 191–204.

    Article  Google Scholar 

  26. M. Smith: “Dissolving metal reductions”, In: R.L. Augustine (Ed.): Reduction. Techniques and Applications in Organic Synthesis, Marcel Dekker, New York, 1968, pp. 95–170.

    Google Scholar 

  27. K. Ismail, S.C. Mitchell, S.D. Brown, C.E. Snape, A.C. Buchanan III, P.F. Britt, D.V. Franco, I.I. Maes, J. Yperman: “Silica-immobilized sulfur compounds as solid calibrants for temperature-programmed reduction and probes for the thermal behavior of organic sulfur forms in fossil fuels”, Energy & Fuels, Vol. 9, (1995), pp. 707–716.

    Article  CAS  Google Scholar 

  28. I.I. Maes, J. Yperman, H. Van den Rul, D.V. Franco, J. Mullens, L.C. Van Poucke, G. Gryglewicz, P. Wilk: “Study of coal-derived pyrite and its conversion products using atmospheric pressure temperature-programmed reduction”, Energy & Fuels, Vol. 9, (1995), pp. 950–955.

    Article  CAS  Google Scholar 

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Kozłowski, M., Wachowska, H. & Yperman, J. Composition of extraction products from alkylated high-sulphur coals. cent.eur.j.chem. 1, 366–386 (2003). https://doi.org/10.2478/BF02475223

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